Process for the manufacture of asphaltic products



April 3, 1934. J. c. BLACK ET A1. 1,953,333

PROCESS FOR THE MANUFACTURE OF ASPHAUTIC PRODUCTS Filed veeg?, 1927 BY w/RTa/e/HL.

. .6 w TTOR EY JOH/V C. BLHC'K.

i time win be of i ..40l qured degree in a Patented Apr. 3, 1934 1,953,333 rRooEss Fon THE MANUFACTUBE oF ASPHALTIC 301m C. Black, Los Angeles,

Watson, Calif., assignors,

PRJDUCTS` and Wirt D. Rial, by mesne assign-A ments, in Earle w. Gard, Palos verdes Estates, caur.

Application December 7, 1927, Serial No. 238,428

12 Claims. (Cl. 19o- 74) i Y phaltic oil to a pointl of cracking or other decomh,` l

Y This invention relates to a process for ktreating asphaltic residuum, and has particular reference to a method for producing a high grade asphalt suitable for any of the various uses in the art.

An object of the invention isto provide asimple, eflcient and economical process by which asphaltic residuum may be converted into an asphaltic product, whichwill have a relatively high melting point and flash, and at the same a suitable ductility.

Another object of the invention is to provide a simple and eilicient process for manufacturing asphaltic products. in which the various characteristics of ductility, high melting point and 15 flash, required by different branches of the individual art, may be controlled, separately or combinedly. Another object of the invention is to provide a method by which asphaltic residuum may be -uniformly oxidized to the required degree .20 at a minimum consumption of time, and with a minimum consumption of the oxidizing agent.

Heretofore, difllculty has been experienced in providing an asphaltic material entirely suitable for the manufacture of roofing felt, battery sealg5 ing compounds, and the like, in which relatively high iiash and high melting point materials are required, and one which will have suitable ductility at 77 degrees F. We have discovered that this is due to producing products which are not uniformly oxidized, in which some part ofthe asphaltic material has been overoxidized, while other parts have not been suiciently oxidized to give the required melting point, 4flash and ductility. We have discovered that these diiculties may be overcome by employing a smaller quantity of air and alonger time contact betweenthe asphaltic oil and the air, in `-`which case a partial oxidizing action is uniformly effected to the re` much shorter time and without the formation of carbonaceous material. 7 In the conventional method of oxidizing asphaltigoils for the production of oxidized asphalt, air is introduced into a cylindrical still containing the asphaltic oil through a spray line and at the same time'the asphaltic oil contained in the still is heated to a temperature sufficient to obtain the oxidizing reaction, approximately 450 to 550 degrecs F. -By such methods the vair is only in contact with the asphaltic oil momentarily, passing upward through the depth of the oil in the still, thence out through the vapor line,. carrying products of distillation, whereby excessive quantities of air must be employed to obtain thedesired product. On account of the short time contact of the air with the asphaltic oilundergoing oxidaf tion, aA uniform oxidized product cannot be obtained, also a uniform temperature is difficult to maintain since the oxidizing reaction is exothermic and the added heat may overheat the as- I 1 on An- MAID- position reaction, thereby renderingthe product more brittle or less ductile than it would be if a `uniform oxidized product at a lower temperature duced, which by our process are conserved and oxidized to desirable asphaltic products. A For example, by the conventional cylindrical batch still method the time required to convert v I 1,953,333 vi UNITED STATES PATENT oFFlcr:

a batch offasphaltic oil to an oxidized product suitable for the manufacture of Vroong felt, rc1 quires approximately 24 hours or more, while by our invention the reaction is accomplished in about one half the time and the total quantity of air employed is approximately vonly 50 per cent of the air required by the conventional batch method.

'In the manufacture of oxidized asphalt for coating roofing felt, or the like, by our invention we may obtain a productl having the following Penetration @77- F p- 15 to 18 Melting point.; g j 225 to 260 F. Ductility 1.25 to2!) cm.

Flash 430 to460 F. v

We have found it advantageous to circulate a large amount oi' oil'through the heating and air contact coil and a relatively small volume of air, the contact being over a prolonged period 'oi' time relative to the time of contactjn a cylindrical still'such as previously'used in the art; by this procedure we are enabled to produce a superior finished asphaltic compound as the oxidation is not as severe carbonaceous material is produced and greater ductility and penetration is obtained at a. given flash and melting point.

We have also found that by maintaining a pressure on the heating and contact coil, oxidation may be hastened, or maintaining adenite rateof oxidation less air may be used; that is to say the air will be more effectively denuded of its oxygen content. 'Ihis will represent a saving in 'compressed air as well as a saving in heat.

With the foregoing preliminary explanation the preferred embodiment of ourl invention will now be more fully explained by reference to the accompanying drawing, which is a diagrammatical representation oi'a preferred apparatus for icarrying out the operations of the present invenion.

In the drawing. Figure 1 represents the complete apparatus for carrying out the invention and Figure 2 shows the cross-section of the still with the result that less Amay be externally heated.

In Figure 1, 1 represents generally a still or chamber for holding the bulk supply of oil, which A pipe 2 connects the still 1 at the bottom to the inlet side of a steam jacketed pump 4 controlledrv by the valve 40. A pipe 8 controlled by the valve 3 is connected to the pipe 2 and leads to a source of asphaltic oil residuum not shown. A pipe 5, controlled by the valve 6 connects the discharge side of the pump 4 to pipe 32. A pipe 18 controlled by the valve 19 is connected to the pipe 32, and leads to a source of steam not shown. A pipe 21, controlled by valve 7 is connected to the pipe 32 and leads to a source of air not shown. The pipe 32l is connected to a heater coil 9 at the top. The heater and air contact coil 9 is interposed in the furnace 10 which is provided with a. burner 1l which leads to a source of fuel not trolledl by the valve 33 connects the heater coil 9 at the bottom to the still 1, passing through the shell of the still 1 near the top. A pipe 12 controlled by the valve 31 connects the pipe 5 to storage tank 13. A pipe 16 controlled bythe valve 1 near the bottom. A pipe valve 36, is connected to the steam into still 1 to a predetermined level by connects the steam p'pe 14 to the still 1 near `the top. The pipe 14 controlled by the valve 34 is connected tothe spray line 17 which is in the still controlled by the pipe 14. The steam pipe 14 leads to a source shown. A vapor line 20 is connected to the still 1 at the top by the pipe fittings 27. The vapors may be taken to a condenser where the condensible materials are condensed by cooling fluid and the uncondensed vapors, gases and steamI are withdrawn by means of a vacuum pump which Will maintain the desired vacuum in the still 1. In Figure 2, which is a cross-section of the still 1 showing the connections of the vapor line 20 to the still 1, 42 is across tting connected to the top of the still bymeans of a nipple 43. The pipe 26 connects the cross fitting 42 to the cross fitting 42'. The -pipe 27 connects the cross fitting 42 to the vapor line 20 by means ofa T. The pipes 33, 32, 2, 12 and 5 are preferably covered with a suitable insulating material to prevent any substantal loss of heat, or they may be steam jacketed.

The preferred process asA carried out inthe apparatus described is as follows:

Asphaltic oil, which maybe any crude petroleum oil or preferably residuum derived by the distillation of an asphalt or mixed base crude petroleum oil, and preferably ranging in gravity from 10 or below to 16 degrees operating pump 4, which takes suction on the charging line 8 through the pipe 2. The charging line 8 leads to a source of supply not shown. During the charging of the still 1, Valve is closed and valve 3 is opened. The petroleum oil stock is discharged by the ypump 4 into the pipe 5,l valve 31 being closed and valve 6 being open. From pipe 5 the petroleum oil stockl passes through the pipe 32, heater coil 9, pipe 33 and valve 33' and then into the still 1, valves 7 and` 19 being closed. When still 1 contains a sufcient charge oi the petroleum oil stock, valve 3 is closed and valve 40 is opened which permits the oilrto circulate from the still 1 through the heating coil 9 and back to the still 1, or source of bulk supply. Heat is now appliedtto the furnace 10 by means of the burner 11 and regulated so that the oil passing through the heater coil 9 will attain a temperature of approximately 450 to 550 degrees F. or whatever temperature is desired for that particular run.

shown. A pipe 33 con-4 B., is charged When the circulating oil has attained a suitable temperature and flash a regulated stream of ar is introduced into the pipe 32 from the pipe 21, which leads to a source of compressed air not shown. In some cases it may be desired to introduce a small amount of air during the charging and heating of the oil.

- The circulation of the oil at the oxidizing temperature and the introduction of the air are maintained for a period of time required to obtain the desired product, such time depending upon the quality ofthe oil employed, the product desired and the amount of air introduced. If desired, the oil and air passing through the heater coil 9 may be kept at any desired pressure above atmospheric, by regulating valve 33'. Also a vacuum may be maintained on the bulk supply chamber-or still 1, whereby the oxidation is carried on at a still further reduced temperature.

In producing certain varieties of oxidized asphalt it may be found advantageous to introduce steam along with the air which is carried out by opening valve 19 suiciently to admit the desired amount of steam from pipe. 18 which decreases the time of reaction, and the tendencyof the oil to crack, thereby producing a product of a superior quality.

Duringthe oxidation of the asphalt with air or steam and air, the air, in conjunction with the products of distillation, passes from the still 1 into the vapor line 20. The vapor line 20 leads to a condenser not shown Where the oil products are condensed and separated from the gases.

When the petroleum oil residuum has been oxidized to the required degree, it is discharged into the storage tank 13 passing from the bottom of the still 1 through the pipe 2, pump 4, pipe 5 and pipe 12, valve 31 being open and valve 6 being closed.

-During the time that the still is being emptied of the finished oxidized asphalt, steam is admitted into the still l through the pipe 16 controlled by the valve 15. `The pipe 16 is connected to the steam pipe 14 which leads to a source of steam not shown. The introduction of steam into the top of still 1 ished products of the still is carried out to prevent explosive mixtures from forming in the top of the still. Therefore the quantity of steam admitted into the still through the pipe 16 is just sucient to ll the space above the liquid asphalt as it is being withdrawn.

In some cases where the oxidized asphaltis not at a suiilciently high flash after the oxidizing operation, the ash may be further raised by steaming the charge for a period of time. This is accomplished by the introduction of steam into the still 1 through the spray line 17 which is connected to the steam line 14 controlled by the valve 34. During this operation, in order to obtain a steam free from water, valve 36 is opened to a slight during the removal of the nextent so as to permit any water to separate from admitted into the heating coil, or steam and air may be intermittently introduced `into the heating coil. The regulation of each depends upon the modifications and changes may be made without` departing from the spirit of the invention and the invention includes all such modications and changes as come within the scope of the vappended claims.

What we claim is:

1. A process of forming oxidized asphalt comprising maintaining a bulk supply of asphaltic oil in a chamber at a pressure not greater than vatmospheric and at a uniform oxidizing temperature, circulating the oil from the bulk supply to and through a heating coil and back to the bulk supply, introducing a regulated stream of air into the circulating oil, passing the oil commingled with air through the coil under a pressure greater than atmospheric and then separating the residual' air with the products of distillation from the 2. A'process of forming oxidized asphalt, comprising, maintaining a bulk supply of asphaltic oil in a chamber at a pressure substantially not greater than atmospheric, maintaining a substantially uniform, oxidizing temperature therein, by continuously circulating the oil fromthe bulk supply to and through a heating coil and back to the bulk supply, continuously introducing a regulated stream of air into the circulating oil before it enters the heating coil and continuously withdrawing the residual air and products of distillation from the chamber.

3. A process of producing asphalt which com- I prises passing a commingled stream of oil and air through a coil, maintaining said coil atv an elevated temperature, maintaining superatmos pheric pressure on said commingled oil and air in said coil, regulating the temperature and pressure and air to produce oxidized asphalt, and reducing the pressure on said oil and air and separating the asphalt from the vapors and gases under said reduced pressure. i

4. A method of producing asphalt which comprises passing a commingledV stream ol oil and air through a coil', maintaining said oil in saidv coil at an elevated' temperature, introducing said commingled stream of heated oil and airinto a bulk supply chamber, separating the oxidized asphalt from the .gases in said bulk supply chamber under vacuum. Y

5. A process oi.' producing asphalt which comprises passing a commingled stream of oil and air through a coil, maintainingsaid coil at an elevatedteinperatura but insufficient to substanreduced pressure.

tially crack said oil, maintaining 'superatmospheric pressureon said commingled oil and air in said coil, .regulating the temperature and'pressure and air to produce oxidized asphalt, and reducing the pressure on said oil and airand separatingthe asphalt from the vapors and gases under said vated temperature, introducing said commingled .maintaining said oil in said coil at an elevated temperature,v4 but insuiiicient to substantially crack said oil, introducing said commingled stream ofv heated oil and air into a chamber maintaining said chamber under vacuum, separating the oxidized asphalt from the gases under vacuum. i

9. A method f producing asphalt which comprises maintaining a bulk supply of oil, circulating oil from said bulk supply introducing air into the circulating oil through a.v coil, maintaining said oil in said coil at anielevated temperature,

introducing said commingled stream of oil and air into said bulk supply chamber, maintaining said chamber under vacuum, separating the gases and oil from the vapors under vacuum in said chamber, removing the oil and gases from said chamber and removing the asphalt from said chamber. V

10. A method of producing asphalt which comprises maintaining a bulk supply of oil, circulating oil from said bulk supply introducing air into the circulating, oil through a coil under ysuper-- atmospheric pressure, maintaining said oil in said coil at an elevated temperature, introducing said commingled stream of oil and air into said bulk supply chamber, maintaining s aid chamber under vacuum, separating the gases and oil from the vapors under vacuum in said chamber, removing the oil and gases from said chamber and removing the asphalt from said chamber.

, 11. A method'of producing asphalt which comprises maintaining a bulk. supply of oil, circulating oil from said bulk supply introducing air into the circulating oil through a coil, maintaining said oil in said .coil at an elevated temperature, but insuflicient to substantially crack said oil, introducing said commingled stream of oil and air into said bulk supply chamber, maintaining said chamber under vacuum, separating the gases and oil from thevapors vunder vacuum in said 12. A methodof producing'asphalt which comprises maintaining ay bulk supply of oil, circulatingioil from said bulk supply introducing air into the- Vcirculating oil through a coil under superatmospheric pressure, maintaining said oil in said coil -'at an"elevatedltemperature, but insuflicient to substantially crack said oil,l introducing said Y i l commingled stream of oil and air into said bulk 6,. A methcd of producing asphalt which comprises passing a commingled stream of oil and air through'a coil under superatmospheric pres` sure, maintaining said coilin said coil at an elesupply chambr, maintaining said chamber under' -.vacuu.m, separating thegases and oil from the vapors under vacuum in `said chamber, removing thev oil and gasesfrom said chamberl and removing the asphaltfrom said chamber.

I .k JOHN C. BLACK.

WIRT D.v 

